CN101914856B - Stripping method of PLA fibre - Google Patents

Stripping method of PLA fibre Download PDF

Info

Publication number
CN101914856B
CN101914856B CN201010255019A CN201010255019A CN101914856B CN 101914856 B CN101914856 B CN 101914856B CN 201010255019 A CN201010255019 A CN 201010255019A CN 201010255019 A CN201010255019 A CN 201010255019A CN 101914856 B CN101914856 B CN 101914856B
Authority
CN
China
Prior art keywords
stripping
liquid
detergent
sodium thiosulfate
pla
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201010255019A
Other languages
Chinese (zh)
Other versions
CN101914856A (en
Inventor
庄小雄
姚登辉
杨国荣
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Textile Academy Shaoxing Jiangnan Branch China Textile Academy Co Ltd
Original Assignee
China Textile Academy Shaoxing Jiangnan Branch China Textile Academy Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Textile Academy Shaoxing Jiangnan Branch China Textile Academy Co Ltd filed Critical China Textile Academy Shaoxing Jiangnan Branch China Textile Academy Co Ltd
Priority to CN201010255019A priority Critical patent/CN101914856B/en
Publication of CN101914856A publication Critical patent/CN101914856A/en
Application granted granted Critical
Publication of CN101914856B publication Critical patent/CN101914856B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Coloring (AREA)
  • Detergent Compositions (AREA)

Abstract

The invention discloses a stripping method of a PLA fibre, belonging to the technical field of after finishing processes of fabrics. The method can be used for processing PLA fabrics in light color or medium deep color and comprises the following steps of: firstly, striping the dye by using sodium thiosulfate or tri-sodium dodecyl sulfate phenyl phosphor and penetrant JFC as the stripping liquid, wherein the adding amount of sodium thiosulfate is 1-10g/L, the adding amount of the tri-sodium dodecyl sulfate phenyl phosphor is 3-20g/L, and the adding amount of the penetrant JFC is 1-10g/L; and then cleaning the dye floating on the surface of the fabrics by using detergent FK-9503, wherein the adding amount of the detergent FK-9503 is 1-10g/L. The invention can realize successful stripping of the PLA fibre fabrics, avoids great damage to the PLA fibre, and solves the problem that the PLA can not be redyed.

Description

The stripping method of PLA fiber
Technical field:
The present invention relates to the stripping method of a kind of PLA (PLA) fiber, belong to after-finishing of textile products technology field.
Background technology:
PLA fiber (polylactic acid) is with starch-containing materials such as corn, Ipomoea batatas, wheats; Be converted into lactic acid through fermentation; The fiber of processing through polymerization, spinning again, it not only has excellent physical property and takes performance, and the ability biodegradation; Being a kind of novel environment friendly fiber of Natural Circulation fully, also is present unique synthetic fiber that do not rely on petroleum resources.
At present, because PLA fibrous glass temperature is lower, and do not have the special-purpose dyestuff of PLA fiber on the market; Because the physicochemical properties that the PLA fiber is unique are in dyeing course, all bigger to the sensitiveness of temperature, pH value, dyestuff; In batch production process, be easy to cause aberration, cylinder poor, do not redye production being caused very big economic loss if do not strip; Because PLA fiber alkali resistance is poor, the stripping method that fibers such as cotton, hair, terylene are commonly used is not suitable for the PLA fiber.
Have based on this, make the present invention.
Summary of the invention:
The objective of the invention is the problem that all the time can't redye to the PLA fiber, remedy the aberration that the PLA fiber occurs easily in dyeing course, cylinder difference problem, thus a kind of stripping method of suitable PLA fiber is provided.
First aspect of the present invention provides a kind of stripping method of PLA fiber; Light fabric is handled; May further comprise the steps: adopt sodium thiosulfate or three pairs of dodecyl sodium sulfate phenyl phosphorus to cooperate penetrating agent JFC to be the liquid of stripping earlier, dyestuff is stripped, wherein the sodium thiosulfate addition is 1~10g/L; Three pairs of dodecyl sodium sulfate phenyl phosphorus additions are 3~20g/L; The penetrating agent JFC addition is 1~10g/L, and then the dyestuff that adapted detergent FK-9503 will float over fabric face cleans, and detergent FK-9503 addition is 1~10g/L.
In the above-mentioned stripping method, cooperate following technological parameter, can make the aforesaid liquid of stripping obtain best treatment effect.
The step 1 of stripping: (90~110 ℃, 5~30min) → heat is washed (80~100 ℃) → detergent and is washed (70~90 ℃) → washing (room temperature) → oven dry to pad the liquid of stripping (one soaks one rolls) → decatize.
The step 2 of stripping: dipping is stripped, and liquid (80~100 ℃, wash (80~100 ℃) → detergent and wash (70~90 ℃) → washing (room temperature) → oven dry by 10~40min) → heat.
Another aspect of the present invention also provides a kind of stripping method that is directed against the PLA fiber of middle deep-colour fabric; May further comprise the steps: adopt the alkylamine polyoxyethylene to be the liquid one of stripping; Alkylamine polyoxyethylene addition is 5~30g/L, in advance dyestuff is carried out part and strips, and then adopt sodium thiosulfate or three pairs of dodecyl sodium sulfate phenyl phosphorus to be the liquid two of stripping; Dyestuff is stripped once more; The sodium thiosulfate addition is 1~10g/L, three couples of dodecyl sodium sulfate phenyl phosphorus 3~20g/L, and then the dyestuff that adapted detergent FK-9503 will float over fabric face is cleaned.
In the above-mentioned stripping method, cooperate following technological parameter, can make the aforesaid liquid of stripping obtain best treatment effect.
The step 1 of stripping: pad (70~102 ℃ of the liquid one of stripping (soaks rolls) → decatize; 10~30min) → washing (room temperature) → (90-110 ℃, 5~20min) → heat is washed (80~100 ℃) → detergent and is washed (70~90 ℃) → washing (room temperature) → oven dry to pad the liquid two of stripping (one soaks one rolls) → decatize.
The step 2 of stripping: dipping is stripped, and liquid one (70~90 ℃, 20~50min) → washing (room temperature) → dipping is stripped, and (80~100 ℃, liquid two is washed (80~100 ℃) → detergent and is washed (70~90 ℃) → washing (room temperature) → oven dry by 10~40min) → heat.
Among the present invention, described penetrating agent JFC and detergent FK-9503 spin the product that chemical inc is produced available from spinning in the Shaoxing in chemical industry Co., Ltd or Beijing.
Further refinement as to technique scheme of the present invention is following:
1: use sodium thiosulfate to cooperate other auxiliary agent in suitable padding under the technology light fabric to be stripped, step is following:
(1) technical recipe:
The liquid of stripping: sodium thiosulfate 5~10g/L
JFC 1~10g/L
Detergent FK-9503:1~10g/L
(2) step of stripping: (90-110 ℃, 5~20min) → heat is washed (80~100 ℃) → detergent and is washed (70~90 ℃) → washing (room temperature) → oven dry to pad the liquid of stripping (one soaks one rolls) → decatize.
2: use sodium thiosulfate to cooperate other auxiliary agent under suitable impregnation technology, light fabric to be stripped, step is following:
(1) technical recipe:
The liquid of stripping: sodium thiosulfate 1~5g/L JFC 1~10g/L
Detergent FK-9503:1~10g/L
(2) step of stripping:
Dipping is stripped, and liquid (80~100 ℃, wash (80~100 ℃) → detergent and wash (70~90 ℃) → washing (room temperature) → oven dry by 10~40min) → heat.
3: use alkylamine polyoxyethylene, sodium thiosulfate to cooperate other auxiliary agent to strip at the suitable centering deep-colour fabric that pads under the technology, step is following:
(1) technical recipe:
The liquid one of stripping: alkylamine polyoxyethylene 10~30g/L
The liquid two of stripping: sodium thiosulfate 5~10g/L JFC 1~10g/L
Detergent: detergent FK-9503 1~10g/L
(2) step of stripping:
Pad (70~102 ℃ of the liquid one of stripping (soaks rolls) → decatize; 10~30min) → washing (room temperature) → (90-110 ℃, 5~20min) → heat is washed (80~100 ℃) → detergent and is washed (70~90 ℃) → washing (room temperature) → oven dry to pad the liquid two of stripping (one soaks one rolls) → decatize.
4: use alkylamine polyoxyethylene, sodium thiosulfate to cooperate other auxiliary agent centering deep-colour fabric under suitable impregnation technology to strip, step is following:
(1) technical recipe:
The liquid one of stripping: alkylamine polyoxyethylene 5~20g/L
The liquid two of stripping: sodium thiosulfate 1~5g/L JFC 1~10g/L
Detergent: detergent FK-9503 1~10g/L
(2) step of stripping:
Dipping is stripped, and liquid one (70~90 ℃, 20~50min) → washing (room temperature) → dipping is stripped, and (80~100 ℃, liquid two is washed (80~100 ℃) → detergent and is washed (70~90 ℃) → washing (room temperature) → oven dry by 10~40min) → heat.
5: use three pairs of dodecyl sodium sulfate phenyl phosphorus to cooperate other auxiliary agent in suitable padding under the technology light fabric to be stripped, step is following:
(1) technical recipe:
The liquid of stripping: three couples of dodecyl sodium sulfate phenyl phosphorus 10~20g/L JFC 1~10g/L
Detergent FK-9503:1~10g/L
(2) step of stripping:
(90-110 ℃, 10~30min) → heat is washed (80~100 ℃) → detergent and is washed (70~90 ℃) → washing (room temperature) → oven dry to pad the liquid of stripping (one soaks one rolls) → decatize.
6: use three pairs of dodecyl sodium sulfate phenyl phosphorus to cooperate other auxiliary agent under suitable impregnation technology, light fabric to be stripped, step is following:
(1) technical recipe:
The liquid of stripping: three couples of dodecyl sodium sulfate phenyl phosphorus 3~10g/L JFC 1~10g/L
Detergent FK-9503:1~10g/L
(2) step of stripping:
Dipping is stripped, and liquid (80~100 ℃, wash (80~100 ℃) → detergent and wash (70~90 ℃) → washing (room temperature) → oven dry by 10~40min) → heat.
7: use alkylamine polyoxyethylene, the three pairs of dodecyl sodium sulfate phenyl phosphorus to cooperate other auxiliary agent to strip at the suitable centering deep-colour fabric that pads under the technology, step is following:
(1) technical recipe:
The liquid one of stripping: alkylamine polyoxyethylene 10~30g/L
Two: three pairs of dodecyl sodium sulfate phenyl of liquid phosphorus, 10~20g/L JFC, 1~10g/L strips
Detergent: detergent FK-9503 1~10g/L
(2) step of stripping:
Pad (70~102 ℃ of the liquid one of stripping (soaks rolls) → decatize; 10~30min) → washing (room temperature) → (90-110 ℃, 5~20min) → heat is washed (80~100 ℃) → detergent and is washed (70~90 ℃) → washing (room temperature) → oven dry to pad the liquid two of stripping (one soaks one rolls) → decatize.
8: use alkylamine polyoxyethylene, three pairs of dodecyl sodium sulfate phenyl phosphorus to cooperate other auxiliary agent centering deep-colour fabric under suitable impregnation technology to strip, step is following:
(1) technical recipe:
The liquid one of stripping: alkylamine polyoxyethylene 5~20g/L
Two: three pairs of dodecyl sodium sulfate phenyl of liquid phosphorus, 3~10g/L JFC, 1~10g/L strips
Detergent: detergent FK-9503 1~10g/L
(2) step of stripping:
Dipping is stripped, and liquid one (70~90 ℃, 20~50min) → washing (room temperature) → dipping is stripped, and (80~100 ℃, liquid two is washed (80~100 ℃) → detergent and is washed (70~90 ℃) → washing (room temperature) → oven dry by 10~40min) → heat.
Technological principle of the present invention:
The invention belongs to dyeing and finishing processing method, it is characterized in that selecting for use a kind of alkalescent to have the chemical assistant of reduction, cooperate suitable technology, under the prerequisite that guarantees the PLA fiber strength, it is stripped.In order to obtain the satisfactory weak base performance is carried out reduction decomposition to PLA fabric dyestuff the chemical assistant that has; We are through test of many times, have filtered out sodium thiosulfate, the three pairs of dodecyl sodium sulfate phenyl phosphorus, these three kinds of materials of alkylamine polyoxyethylene at last.Adopt the combination of these three kinds of materials to cooperate i.e. success the PLA fabric is stripped of suitable technology, avoided again the PLA fiber is caused too big strength damage, solved the problem that PLA can not redye.
The present invention compared with prior art has following outstanding advantage and good effect:
1, because the PLA fiber has not alkaline-resisting; Not acidproof; Powerful oxidation corrosion resistance not, the character of anti-strong reduction not, that the present invention has improved is cotton, hair, the fabric technology that strong reductant such as a large amount of caustic soda of adopting, soda ash, sodium hydrosulfite, clorox, hydrogen peroxide solution, acetic acid and oxidant strip of stripping such as wash; Filter out two kinds of chemical assistants, avoided the strength damage of PLA fiber with dyestuff on the weak base performance reduction decomposition PLA fiber.
2, this stripping method of confirming through test of many times has been retrieved because the enormous economic loss that zein fiber aberration occurs easily to be brought plays an important role to improving the whole dyeing and finishing processing method of PLA fiber.
Below in conjunction with the specific embodiment the present invention is described further.
The specific embodiment:
Embodiment 1: the yellow PLA fabric of light color is padded strip
(1) technical recipe:
The liquid of stripping: sodium thiosulfate 5g/L JFC 5g/L
Detergent FK-9503:5g/L
(2) step of stripping:
Pad the liquid of stripping (one soaks one rolls) → decatize (95 ℃, 10min) → heat wash (90 ℃) → detergent wash (75 ℃) → washing (room temperature) → oven dry.
Embodiment 2: the blue PLA fabric of light color is flooded strip
(1) technical recipe:
The liquid of stripping: sodium thiosulfate 1.5g/L JFC 1g/L
Detergent FK-9503:2g/L
(2) step of stripping:
The dipping strip liquid (85 ℃, 25min) → heat wash (85 ℃) → detergent wash (85 ℃) → washing (room temperature) → oven dry.
Embodiment 3: the pink PLA fabric of dark color is padded strip
(1) technical recipe:
The liquid one of stripping: alkylamine polyoxyethylene 25g/L
The liquid two of stripping: sodium thiosulfate 8g/L JFC 8g/L
Detergent: detergent FK-9503 9g/L
(2) step of stripping:
Pad the liquid one of stripping (one soaks one rolls) → decatize (98 ℃, 20min) → washing (room temperature) → the pad liquid two of stripping (one soaks one rolls) → decatize (98 ℃, 10min) → heat washes (90 ℃) → detergent and wash (85 ℃) → washing (room temperature) → oven dry.
Embodiment 4: centering look blue PLA fabric floods strips
(1) technical recipe:
The liquid one of stripping: alkylamine polyoxyethylene 10g/L
The liquid two of stripping: sodium thiosulfate 4g/L JFC 3g/L
Detergent: detergent FK-9503 6g/L
(2) step of stripping:
The dipping strip liquid one (80 ℃, 40min) → washing (room temperature) → dipping strip liquid two (95 ℃, 25min) → heat wash (95 ℃) → detergent wash (80 ℃) → washing (room temperature) → oven dry.
Embodiment 5: the blue PLA fabric of light color is padded strip
(1) technical recipe:
The liquid of stripping: three couples of dodecyl sodium sulfate phenyl phosphorus 12g/L JFC 5g/L
Detergent FK-9503:3g/L
(2) step of stripping:
Pad the liquid of stripping (one soaks one rolls) → decatize (102 ℃, 10min) → heat wash (80 ℃) → detergent wash (70 ℃) → washing (room temperature) → oven dry.
Embodiment 6: the blue PLA fabric of light color is flooded strip
(1) technical recipe:
The liquid of stripping: three couples of dodecyl sodium sulfate phenyl phosphorus 3g/L JFC 2g/L
Detergent FK-9503:3g/L
(2) step of stripping:
The dipping strip liquid (95 ℃, 30min) → heat wash (80 ℃) → detergent wash (85 ℃) → washing (room temperature) → oven dry.
Embodiment 7: Dark grey PLA fabric is flooded strip
(1) technical recipe:
The liquid one of stripping: alkylamine polyoxyethylene 30g/L
Two: three pairs of dodecyl sodium sulfate phenyl of liquid phosphorus 20g/L JFC 6g/L strips
Detergent: detergent FK-9503 1~10g/L
(2) step of stripping:
Pad the liquid one of stripping (one soaks one rolls) → decatize (102 ℃, 10min) → washing (room temperature) → the pad liquid two of stripping (one soaks one rolls) → decatize (110 ℃, 10min) → heat washes (95 ℃) → detergent and wash (90 ℃) → washing (room temperature) → oven dry.
Embodiment 8: black PLA fabric is flooded strip
(1) technical recipe:
The liquid one of stripping: alkylamine polyoxyethylene 15g/L
Two: three pairs of dodecyl sodium sulfate phenyl of liquid phosphorus 8g/L JFC 5g/L strips
Detergent: detergent FK-9503 10g/L
(2) step of stripping:
The dipping strip liquid one (80 ℃, 50min) → washing (room temperature) → dipping strip liquid two (100 ℃, 20min) → heat wash (90 ℃) → detergent wash (85 ℃) → washing (room temperature) → oven dry.
Among the embodiment 1~8, through detecting, the strong damage of the PLA fiber after stripping is controlled at below 10%, and it is clean to strip, and whiteness can satisfy redying requirement fully more than 70.
The above embodiments of the present invention are can not limit the present invention to explanation of the present invention, in implication suitable with claims of the present invention and any change and the combination in the scope, all should think in the scope of claims.

Claims (2)

1. the stripping method of a PLA fiber; It is characterized in that, use alkylamine polyoxyethylene, sodium thiosulfate centering deep-colour fabric to strip, may further comprise the steps: adopt the alkylamine polyoxyethylene to be the liquid one of stripping; In advance dyestuff being carried out part strips; And then adopt sodium thiosulfate for the liquid two of stripping, dyestuff is stripped once more, and then adapted detergent FK-9503 will to float over the dyestuff of fabric face clean:
(1) technical recipe:
The liquid one of stripping: alkylamine polyoxyethylene 10~30g/L,
The liquid two of stripping: sodium thiosulfate 5~10g/L, JFC 1~10g/L,
Detergent: detergent FK-95031~10g/L;
(2) step of stripping:
Adopt one soak one roll pad the liquid one of stripping → washing → employing one under 70~102 ℃ of following decatize 10~30min → room temperatures soak one roll pad the following heat of the liquid two → 90-110 ℃ of following decatize 5~20min that strip → 80~100 ℃ and wash → wash with detergent under 70~90 ℃ → room temperature under washing → oven dry.
2. the stripping method of a PLA fiber; It is characterized in that, use alkylamine polyoxyethylene, sodium thiosulfate centering deep-colour fabric to strip, may further comprise the steps: adopt the alkylamine polyoxyethylene to be the liquid one of stripping; In advance dyestuff being carried out part strips; And then adopt sodium thiosulfate for the liquid two of stripping, dyestuff is stripped once more, and then adapted detergent FK-9503 will to float over the dyestuff of fabric face clean:
(1) technical recipe:
The liquid one of stripping: alkylamine polyoxyethylene 5~20g/L,
The liquid two of stripping: sodium thiosulfate 1~5g/L, JFC 1~10g/L,
Detergent: detergent FK-95031~10g/L;
(2) step of stripping:
70~90 ℃ down dipping strip under liquid one 20~50min → room temperature → 80~100 ℃ of washings down dipping strip liquid 2 10~40min → 80~100 ℃ following heat wash → 70~90 ℃ with detergent wash → room temperature under washing → oven dry.
CN201010255019A 2010-08-12 2010-08-12 Stripping method of PLA fibre Expired - Fee Related CN101914856B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201010255019A CN101914856B (en) 2010-08-12 2010-08-12 Stripping method of PLA fibre

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201010255019A CN101914856B (en) 2010-08-12 2010-08-12 Stripping method of PLA fibre

Publications (2)

Publication Number Publication Date
CN101914856A CN101914856A (en) 2010-12-15
CN101914856B true CN101914856B (en) 2012-10-17

Family

ID=43322481

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201010255019A Expired - Fee Related CN101914856B (en) 2010-08-12 2010-08-12 Stripping method of PLA fibre

Country Status (1)

Country Link
CN (1) CN101914856B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103255643B (en) * 2013-05-21 2015-05-13 如皋市协和印染有限公司 Three-protection fabric color changing method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3336012B2 (en) * 1992-10-21 2002-10-21 テンセル リミティド Fiber processing
CN101195968A (en) * 2007-12-13 2008-06-11 常熟理工学院 High temperature dyeing and printing colour stripping process method for dacron
CN101492889A (en) * 2009-02-24 2009-07-29 天津工业大学 Dyeing defect renovation agent and method for preparing the same
CN101787644A (en) * 2010-03-10 2010-07-28 苏州大学 Stripping processing method of textile printing defective items

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3336012B2 (en) * 1992-10-21 2002-10-21 テンセル リミティド Fiber processing
CN101195968A (en) * 2007-12-13 2008-06-11 常熟理工学院 High temperature dyeing and printing colour stripping process method for dacron
CN101492889A (en) * 2009-02-24 2009-07-29 天津工业大学 Dyeing defect renovation agent and method for preparing the same
CN101787644A (en) * 2010-03-10 2010-07-28 苏州大学 Stripping processing method of textile printing defective items

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JP特许第3336012号B2 2002.08.02

Also Published As

Publication number Publication date
CN101914856A (en) 2010-12-15

Similar Documents

Publication Publication Date Title
El Shafie et al. One-step process for bio-scouring and peracetic acid bleaching of cotton fabric
CN102080331B (en) Process for pre-treating fabrics by bio-enzymatic method
CN110453510B (en) Composite reducing agent and reduction dyeing method
WO1992018687A1 (en) Removal of excess dye from new textiles
CN103469538B (en) Low-temperature less-alkali pretreatment method for modified polyester/cotton blended knitted fabric
CN111172791B (en) Enzyme dyeing one-bath dyeing process for cotton fabric
CN106638053A (en) One-bath dyeing technology for polyester-cotton blended fabric by natural vegetable dye
CN101914856B (en) Stripping method of PLA fibre
KR101844917B1 (en) Method for Dyeing Artificial Leather
CN114836971B (en) Jean fabric washing method and jean fabric
CN109594357A (en) A kind of cotton plain color shell-fabric dyeing and finishing processing method
KR100785827B1 (en) Bio-towel using enzyme scouring and manufacturing method thereof
CN115110322A (en) Printing and dyeing process of polyester-nylon-viscose blended fabric
CN104532624A (en) Fabric decoloring method
JP4020658B2 (en) Method for dyeing fiber structure and dyed fiber structure
CN102454118A (en) Method for ecologically dyeing yarn
KR101985468B1 (en) method for dyeing artificial leather having melange appearance
CN104746330A (en) Cotton fabric ecological pretreatment new technology
CN113638218B (en) Short-process high-color-fastness improving method for polyester fabric
CN102168387B (en) Method for efficiently stripping fluorescent bleaching and dyeing dyestuff
Islam et al. Effect of chemical dosing amount in conventional cotton fabric pretreatment process
CN115110305A (en) Flax fiber cone yarn bleaching process
Hamzah et al. Conventional and single-step pretreatment process of cotton woven fabric
Padaki et al. Preparatory chemical processes and recent developments
Padaki et al. 8 Preparatory Chemical

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20121017

Termination date: 20160812